Sodium Acetate → 3,3,3-Trifluoro-2-oxopropanal (4-chloro-2-fluoro-5-hydroxyphenylhydrazone)

HRID 984783

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HRID 984783 반응식
C([O-])(=O)C.[Na+].Br[CH:7](Br)[C:8]([C:10]([F:13])([F:12])[F:11])=[O:9].Cl.[F:16][C:17]1[CH:22]=[C:21]([Cl:23])[C:20]([OH:24])=[CH:19][C:18]=1[NH:25][NH2:26]>O>[Cl:23][C:21]1[C:20]([OH:24])=[CH:19][C:18]([NH:25][N:26]=[CH:7][C:8](=[O:9])[C:10]([F:13])([F:12])[F:11])=[C:17]([F:16])[CH:22]=1

참가 물질

5

반응물 3

HCID 517045Sodium AcetateHCID 5505231,1-Dibromo-3,3,3-trifluoroacetoneHCID 691421062-Fluoro-4-chloro-5-hydroxyphenylhydrazine hydrochloride

생성물 1

HCID 691427153,3,3-Trifluoro-2-oxopropanal (4-chloro-2-fluoro-5-hydroxyphenylhydrazone)수율 82.9%

시약·촉매·용매 1

HCID 962Water용매

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온도
90 °C

실험 절차

Then, 49.2 g of sodium acetate and 40.5 g of 1,1-dibromo-3,3,3-trifluoroacetone were dissolved in 400 ml of water, and the solution was heated at 80′ to 90° C. for 40 minutes. The solution was cooled to 0° C. to which 75 g of the crude 2-fluoro-4-chloro-5-hydroxyphenylhydrazine hydrochloride crystals obtained above was added, and the mixture was stirred at room temperature for 70 minutes. The precipitated crystals were collected by filtration and dried under reduced pressure, which afforded 35.4 g of 3,3,3-trifluoro-2-oxopropanal 1-(4-chloro-2-fluoro-5-hydroxyphenylhydrazone).

후처리

  1. customobtained
  2. additionabove was added
  3. filtrationThe precipitated crystals were collected by filtration
  4. customdried under reduced pressure, which

출처 및 근거

ORD 기록
ord-b6f788a001cf4bd3a656af374333efcd
출처 데이터셋
uspto-grants-2005_03
특허 번호
US06869913B1

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